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17 results on '"Laurent Gonon"'

1. Unveiling the multiscale morphology of chemically stabilized proton exchange membranes for fuel cells by means of Fourier and real space studies

Author

Stéphanie Pouget, Lionel Porcar, Pierre-Henri Jouneau, Vincent H. Mareau, Laurent Gonon, Hakima Mendil-Jakani, João Paulo Cosas Fernandes, and Natacha Huynh

Subjects
Materials science, Nanostructure, General Engineering, Ionic bonding, Proton exchange membrane fuel cell, Bioengineering, 02 engineering and technology, General Chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Atomic and Molecular Physics, and Optics, 0104 chemical sciences, Amorphous solid, chemistry.chemical_compound, Membrane, Chemical engineering, chemistry, Phase (matter), Ionic conductivity, General Materials Science, 0210 nano-technology, Ionomer
Abstract

We recently presented the elaboration and functional properties of a new generation of hybrid membranes for PEMFC applications showing promising performances and durability. The strategy was to form, inside a commercial sPEEK membrane, via in situ sol–gel (SG) synthesis, a reactive SG phase able to reduce oxidative species generated during FC operation. In order to understand structure-properties interplay, we use a combination of direct space (AFM/3D FIB-SEM) and reciprocal space (SANS/WAXS) techniques to cover dimensional scales ranging from a hundred to few nanometers. AFM modulus images showed the SG phase distributed into spherical domains whose size increases with the SG uptake (ca. 100–200 nm range). Using contrast variation SANS, we observed that the sPEEK nanostructure is mostly unaffected by the insertion of the SG phase which presents a fractal-like multiscale structure. Additionally, the size of both the particles (aggregates/primary) is much too large to be sequestered in the ionic pathways of sPEEK. These findings indicate that the SG-NPs mainly grow within the amorphous interbundle domains. Noticeable rightward shift and widening of the ionomer peak are observed with the SG content, suggesting ion channel compression and greater heterogeneity of the ionic domain size. The SG phase develops in the interbundle regions with a limited impact on the water uptake but leading to a discontinuity of ionic conductivity. This Fourier and real spaces study clarifies the structure of the hybrid membranes and brings into the question the ideal distribution/localization of the SG phase to optimize the membrane's stabilization.

Published
2021

2. Elaboration and characterization of a 200 mm stretchable and flexible ultra-thin semi-conductor film

Author

Pierre Montmeat, Vincent H. Mareau, M Zussy, Laurent Gonon, C. Castan, L.G. Michaud, Samuel Tardif, F. Fournel, François Rieutord, Département Plate-Forme Technologique (DPFT), Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Synthèse, Structure et Propriétés de Matériaux Fonctionnels (STEP ), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), Département Interfaces pour l'énergie, la Santé et l'Environnement (DIESE), Nanostructures et Rayonnement Synchrotron (NRS ), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and ANR-16-CE92-0024,XMicroFatigue,Etude de l'endommagement en fatigue à l'aide de la microscopie à diffraction Laue des rayons X.(2016)

Subjects
Materials science, thin film, Bioengineering, 02 engineering and technology, Substrate (electronics), 010402 general chemistry, 01 natural sciences, [SPI.MAT]Engineering Sciences [physics]/Materials, Monocrystalline silicon, [PHYS.MECA.MEMA]Physics [physics]/Mechanics [physics]/Mechanics of materials [physics.class-ph], Polymer substrate, General Materials Science, Wafer, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, Electrical and Electronic Engineering, Composite material, Thin film, laue microdiffraction, chemistry.chemical_classification, Mechanical Engineering, strained silicon, Strained silicon, General Chemistry, Polymer, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Grinding, chemistry, Mechanics of Materials, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0210 nano-technology
Abstract

International audience; We describe a process for transferring a 200 nm thick, 200 mm wide monocrystalline silicon (mono c-Si) thin film from a silicon-on-insulator onto a flexible polymer substrate. The result is a stretchable and flexible ultra-thin semiconductor film that can be subjected to tensile stress experiments. The process uses off-the-shelf 200 mm wafers and standard polymer temporary bonding techniques. The backside substrate and buried oxide are removed using grinding and wet etching processes. No cracks or wrinkles are observed on the film prior to the tensile stress experiments. The stretching of the flexible structure results in up to 1.5% uniaxial tensile elastic strain on the thin mono c-Si film.

Published
2019

3. New insights on the compatibilization of PA6/ABS blends: A co-localized AFM-Raman study

Author

Vincent H. Mareau, Lucas Daniel Chiba de Castro, Laurent Gonon, J.P. Cosas Fernandes, and Luiz Antonio Pessan

Subjects
Toughness, Materials science, Polymers and Plastics, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, law.invention, symbols.namesake, chemistry.chemical_compound, Brittleness, law, Phase (matter), Materials Chemistry, Crystallization, chemistry.chemical_classification, Organic Chemistry, Polymer, Compatibilization, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Characterization (materials science), chemistry, Chemical engineering, symbols, 0210 nano-technology, Raman spectroscopy
Abstract

Polyamides belong to the major class of engineering polymers with very attractive properties but fail in a brittle manner under stress concentrators. PA6/ABS blends are well-established commercial materials due to their stiffness/toughness balance even when stress concentrators are present. The pair PA6/ABS is immiscible and exhibits poor mechanical properties due to unfavorable interactions, thus, an efficient compatibilization is mandatory for practical applications. Deep understanding of the processing-structure-properties interplays requires multiple characterization techniques to provide insights on the impact of the processing/compatibilization on morphology and phases' distribution. In this work an advanced co-localized AFM-Raman strategy was used to study the compatibilization of PA6/ABS blends with SAN-g-Maleic Anhydride. AFM and TEM allowed nanomechanical analysis and characterization of the blends' morphologies. Co-localized AFM-Raman provided new fundamental insights on the compatibilizer's effect on the PA6's γ polymorphic crystallization. The amount and distribution of this γ phase were found to depend on the blending protocol.

Published
2018

4. AFM-Raman colocalization setup: Advanced characterization technique for polymers

Author

Vincent H. Mareau, Laurent Gonon, and J.P. Cosas Fernandes

Subjects
chemistry.chemical_classification, Materials science, Polymers and Plastics, Cryoultramicrotomy, Atomic force microscopy, General Chemical Engineering, 010401 analytical chemistry, Colocalization, Nanotechnology, 02 engineering and technology, Polymer, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Analytical Chemistry, Characterization (materials science), symbols.namesake, chemistry, symbols, 0210 nano-technology, Raman spectroscopy
Abstract

The optimization of manufacturing processes and the investigation of polymer materials during their life cycle imply an extended knowledge of the physical and chemical properties of the material. T...

Published
2017

5. Operando Raman Spectroscopy and Synchrotron X-ray Diffraction of Lithiation/Delithiation in Silicon Nanoparticle Anodes

Author

Pascale Bayle-Guillemaud, Gérard Gebel, Ekaterina Pavlenko, Vincent H. Mareau, Manuel Maréchal, Jean-Sébastien Micha, Samuel Tardif, François Rieutord, Laurent Gonon, Sandrine Lyonnard, Maxime Boniface, Lucille Quazuguel, Nanostructures et Rayonnement Synchrotron (NRS ), Modélisation et Exploration des Matériaux (MEM), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Synthèse, Structure et Propriétés de Matériaux Fonctionnels (STEP), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Laboratoire d'Etude des Matériaux par Microscopie Avancée (LEMMA ), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG)

Subjects
Diffraction, Materials science, Silicon, Analytical chemistry, General Physics and Astronomy, chemistry.chemical_element, Nanoparticle, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, law.invention, [PHYS.MECA.MEMA]Physics [physics]/Mechanics [physics]/Mechanics of materials [physics.class-ph], Stress (mechanics), symbols.namesake, Thermal conductivity, law, General Materials Science, Crystalline silicon, ComputingMilieux_MISCELLANEOUS, General Engineering, 021001 nanoscience & nanotechnology, [PHYS.PHYS.PHYS-GEN-PH]Physics [physics]/Physics [physics]/General Physics [physics.gen-ph], Synchrotron, 0104 chemical sciences, chemistry, symbols, 0210 nano-technology, Raman spectroscopy
Abstract

Operando Raman spectroscopy and synchrotron X-ray diffraction were combined to probe the evolution of strain in Li-ion battery anodes made of crystalline silicon nanoparticles. The internal structure of the nanoparticles during two discharge/charge cycles was evaluated by analyzing the intensity and position of Si diffraction peaks and Raman TO-LO phonons. Lithiation/delithiation of the silicon under limited capacity conditions triggers the formation of "crystalline core-amorphous shell" particles, which we evidenced as a stepwise decrease in core size, as well as sequences of compressive/tensile strain due to the stress applied by the shell. In particular, we showed that different sequences occur in the first and the second cycle, due to different lithiation processes. We further evidenced critical experimental conditions for accurate operando Raman spectroscopy measurements due to the different heat conductivity of lithiated and delithiated Si. Values of the stress extracted from both operando XRD and Raman are in excellent agreement. Long-term ex situ measurements confirmed the continuous increase of the internal compressive strain, unfavorable to the Si lithiation and contributing to the capacity fading. Finally, a simple mechanical model was used to estimate the sub-nanometer thickness of the interfacial shell applying the stress on the crystalline core. Our complete operando diagnosis of the strain and stress in SiNPs provides both a detailed scenario of the mechanical consequences of lithiation/delithiation in SiNP and also experimental values that are much needed for the benchmarking of theoretical models and for the further rational design of SiNP-based electrodes.

Published
2017

6. Optimization of hydrophilic/hydrophobic phase separation in sPEEK membranes by hydrothermal treatments

Author

I. Zamanillo Lopez, Vincent H. Mareau, Hakima Mendil-Jakani, and Laurent Gonon

Subjects
chemistry.chemical_classification, Materials science, Small-angle X-ray scattering, General Physics and Astronomy, 02 engineering and technology, Polymer, Conductivity, 010402 general chemistry, 021001 nanoscience & nanotechnology, Microstructure, 01 natural sciences, Hydrothermal circulation, 0104 chemical sciences, chemistry.chemical_compound, Membrane, chemistry, Chemical engineering, Nafion, Polymer chemistry, medicine, Physical and Theoretical Chemistry, Swelling, medicine.symptom, 0210 nano-technology
Abstract

Via SAXS, herein, we studied how a sPEEK microstructure evolves when it is immersed in water at a wide range of temperatures (20-100 °C) and time scales (from a few hours to dozens of days). In particular, we scrutinized the behavior of sPEEK at the temperature and time associated with the appearance of a well-defined nanosegregated morphology. At 80 °C, we observed nanoscale swelling along with smoothing of the water/polymer interface over a long period of time (several days). Herein, two of the main membrane properties, i.e., water uptake and proton conductivity, were studied for different immersion times and temperatures. It was found that the abovementioned properties were remarkably correlated with the evolution of the membrane microstructure, which was partly conserved after drying. The present findings helped us to understand that the thermally activated evolutions observed at both the nanoscale and macroscale were associated with the sPEEK β-relaxation crossover. Therefore, the very different swelling behaviors of sPEEK and Nafion are correlated to the much higher β-relaxation of sPEEK vs. Nafion (75 °C vs. -20 °C - dry state). From a practical viewpoint, this study emphasizes, for membranes alternative to Nafion, the importance and impact of the membrane pretreatment on their functional properties.

Published
2017

7. Morphology-induced percolation in crosslinked AMPS/Fluorolink for fuel cell membrane application

Author

Eliane Espuche, Laurent Gonon, Vincent H. Mareau, Linda Chikh, Odile Fichet, Sylvain Magana, Fabrice Gouanvé, Nicolas Festin, Arnaud Morin, Sandrine Lyonnard, Matthieu Fumagalli, Laboratoire de Physico-chimie des Polymères et des Interfaces (LPPI), Fédération INSTITUT DES MATÉRIAUX DE CERGY-PONTOISE (I-MAT), Université de Cergy Pontoise (UCP), Université Paris-Seine-Université Paris-Seine-Université de Cergy Pontoise (UCP), Université Paris-Seine-Université Paris-Seine, Ingénierie des Matériaux Polymères (IMP), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Synthèse, Structure et Propriétés de Matériaux Fonctionnels (STEP), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), ANR-11-RMNP-0007,MAMEIRIP,MAtériaux Multicouches Echangeurs d'Ions à base de Réseaux Interpénétrés de Polymères(2011), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon, Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)

Subjects
Materials science, Filtration and Separation, 02 engineering and technology, Sulfonic acid, Conductivity, 010402 general chemistry, 01 natural sciences, Biochemistry, Oligomer, chemistry.chemical_compound, Nafion, Polymer chemistry, General Materials Science, Physical and Theoretical Chemistry, ComputingMilieux_MISCELLANEOUS, chemistry.chemical_classification, Polymer, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Membrane, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Chemical engineering, Percolation, Chemical stability, 0210 nano-technology
Abstract

New proton-conducting co-networks were synthesized, characterized and tested as Polymer Exchange Membranes for Fuel Cells application. The membranes were obtained from 2-acrylamido-2-methylpropane sulfonic acid (AMPS) copolymerized with a perfluoropolyether oligomer used as crosslinker (Fluorolink ® FMD700). The structure, the thermo-mechanical behavior, the transport properties and the stability were examined in function of the co-network composition, e.g. increasing amount of conductive AMPS. High proton conductivity (1.10 –3 –5.10 −3 S cm −1 ) was reached at a threshold composition of 10 wt% AMPS, which also corresponds to a significant increase in water sorption. The efficiency of proton transfer was shown to directly correlate to the phase-separated nanostructures. On increasing the AMPS content, hydrophilic clusters embedded in the mechanically-robust FMD700 percolate and a co-continuous 3D morphology is formed. Fuel cells tests performed using the high-AMPS content crosslinked membranes showed behaviors comparable to benchmark Nafion ® under similar conditions, with performances significantly improved when the temperature is increased.

Published
2017

8. Nanocomposite based on functionalized gold nanoparticles and sulfonated poly(ether ether ketone) membranes: Synthesis and characterization

Author

Ilaria Fratoddi, Francesca A. Scaramuzzo, Chiara Battocchio, Laura Fontana, Laurent Gonon, Vincent H. Mareau, Laura Carlini, Maria Vittoria Russo, Iole Venditti, Venditti, Iole, Fontana, Laura, Scaramuzzo, Francesca A., Russo, Maria Vittoria, Battocchio, Chiara, Carlini, Laura, Gonon, Laurent, Mareau, Vincent H., and Fratoddi, Ilaria

Subjects
Materials science, Gold nanoparticle, Nanoparticle, Ether, 02 engineering and technology, fluid cell, 010402 general chemistry, 01 natural sciences, lcsh:Technology, Article, proton exchange membranes, Proton exchange membrane, chemistry.chemical_compound, sulfonated poly(ether ether ketone) membranes, Atomic force microscopy, Polymer chemistry, Water environment, General Materials Science, Surface plasmon resonance, metal nanoparticles, lcsh:Microscopy, lcsh:QC120-168.85, Nanocomposite, atomic force microscopy, lcsh:QH201-278.5, lcsh:T, Fluid cell, Gold nanoparticles, Metal nanoparticles, Proton exchange membranes, Sulfonated poly(ether ether ketone) membranes, Materials Science (all), 021001 nanoscience & nanotechnology, 0104 chemical sciences, Sulfonate, Membrane, chemistry, Chemical engineering, Colloidal gold, lcsh:TA1-2040, gold nanoparticles, lcsh:Descriptive and experimental mechanics, lcsh:Electrical engineering. Electronics. Nuclear engineering, 0210 nano-technology, lcsh:Engineering (General). Civil engineering (General), lcsh:TK1-9971, Metal nanoparticle, Sulfonated poly(ether ether ketone) membrane
Abstract

Gold nanoparticles, capped by 3-mercapto propane sulfonate (Au-3MPS), were synthesized inside a swollen sulfonated poly(ether ether ketone) membrane (SPEEK). The formation of the Au-3MPS nanoparticles in the swollen sPEEK membrane was observed by spectroscopic and microscopic techniques. The nanocomposite containing the gold nanoparticles grown in the sPEEK membrane, showed the plasmon resonance λmax at about 520 nm, which remained stable over a testing period of three months. The size distribution of the nanoparticles was assessed, and the sPEEK membrane roughness, both before and after the synthesis of nanoparticles, was studied by AFM. The XPS measurements confirm Au-3MPS formation in the sPEEK membrane. Moreover, AFM experiments recorded in fluid allowed the production of images of the Au-3MPSatsPEEK composite in water at different pH levels, achieving a better understanding of the membrane behavior in a water environment; the dynamic hydration process of the Au-3MPSatsPEEK membrane was investigated. These preliminary results suggest that the newly developed nanocomposite membranes could be promising materials for fuel cell applications.

Published
2017

9. Impact of gas stoichiometry on water management and fuel cell performance of a sulfonated Poly(Ether Ether Ketone) membrane

Author

Arnaud Morin, Pauline Legrand, Laurent Gonon, and Vincent H. Mareau

Subjects
Water transport, Hydrogen, Renewable Energy, Sustainability and the Environment, Water flow, Energy Engineering and Power Technology, chemistry.chemical_element, Proton exchange membrane fuel cell, Dielectric spectroscopy, chemistry.chemical_compound, Membrane, chemistry, Chemical engineering, Nafion, Polymer chemistry, Electrical and Electronic Engineering, Physical and Theoretical Chemistry, Stoichiometry
Abstract

Fuel cell tests have been performed on sulfonated Poly(Ether Ether Ketone) (sPEEK) membranes using dry gases. Impact of gas stoichiometry on performance evolution and membrane–electrodes assembly's water distribution optimization (water management) was studied. During the tests, output voltage evolution was recorded as well as impedance spectra, polarization curves and water amount collected at both sides. Fuel cell performances were observed to be influenced by water management which depends on both operating conditions and membrane intrinsic properties. Increasing either hydrogen or oxygen stoichiometry leads to a decrease of performance. This effect was more pronounced for hydrogen increase (anode). This has been ascribed to a global drying of the membrane along with the appearance of a heterogeneous hydration both through the MEA and along the gas channels. Cell performance characterization during the membrane lifespan was mainly based on Electrochemical Impedance Spectroscopy measurements and showed that water distribution heterogeneity increased with operating time for sPEEK membrane, leading to a drop of performance. This was mainly ascribed to the drying of the gas inlet and the increased hydration at the gas outlet. These behaviours were not observed for the better performing Nafion, which underlines the impact of membrane water transport properties on fuel cell performance.

Published
2012

10. Synthesis and characterization of ionic conducting sulfonated polybenzimidazoles

Author

Vincent Martin, Gérard Gebel, Julien Jouanneau, Laurent Gonon, Régis Mercier, Matériaux organiques à propriétés spécifiques (LMOPS), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI ), Institut de Chimie du CNRS (INC)-Institut National Polytechnique de Grenoble (INPG)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut National Polytechnique de Grenoble (INPG)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Institut Nanosciences et Cryogénie (INAC), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
chemistry.chemical_classification, Condensation polymer, Polymers and Plastics, Chemistry, Organic Chemistry, Ionic bonding, 02 engineering and technology, Polymer, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Polyelectrolyte, polybenzimidazole polyether polysulfone membrane proton fuel cell Ionic conductivity Ionomers Solubility Thermal stability, 0104 chemical sciences, chemistry.chemical_compound, [CHIM.POLY]Chemical Sciences/Polymers, Polymer chemistry, Materials Chemistry, Copolymer, Ionic conductivity, Solubility, 0210 nano-technology, Benzoic acid
Abstract

By copolymerization of the disodium-2,2′-disulfonate-4,4′-oxydibenzoic acid (SODBA), the 4,4′-oxybis(benzoic acid) (OBBA) with the bis 3,4-(diaminophenyl)sulfone (BDAPS), a series of high molecular weight sulfonated polybenzimidazoles (sPBI) were prepared by varying the ratio of monomers SODBA/OBBA. Polymers with ion exchange capacity (IEC) ranging from 0 to 3.2 meqH+/g were obtained. The chemical structure of the sPBI was confirmed by NMR, Fourier-transform infra-red (FTIR). Although the sPBI display a very poor solubility in organic solvents, they are, in the ammonium salt form, soluble in polar aprotic solvents such as DMF, NMP, or DMSO. Tough and ductile membranes from solution casting method were prepared. The water uptake and the ionic conductivity were determined at 30 and 90 °C. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 1732–1742, 2010

Published
2010

11. Synthesis of Sulfonated Polybenzimidazoles from Functionalized Monomers: Preparation of Ionic Conducting Membranes

Author

Gérard Gebel, Julien Jouanneau, and Laurent Gonon, Régis Mercier, Matériaux organiques à propriétés spécifiques (LMOPS), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI ), Institut de Chimie du CNRS (INC)-Institut National Polytechnique de Grenoble (INPG)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut National Polytechnique de Grenoble (INPG)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Institut Nanosciences et Cryogénie (INAC), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Thermogravimetric analysis, Polymers and Plastics, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Inorganic Chemistry, chemistry.chemical_compound, Ionic conductivity, Polymer chemistry, Materials Chemistry, Copolymer, Thermal stability, Fourier transform infrared spectroscopy, chemistry.chemical_classification, Chemistry, Comonomer, Organic Chemistry, Polymer chains, nonbiological, Polymer, 021001 nanoscience & nanotechnology, 0104 chemical sciences, sulfonated polybenzimidazole Polysulfones synthesis membrane, [CHIM.POLY]Chemical Sciences/Polymers, Membrane, Polymerization, 0210 nano-technology
Abstract

In the present work, a new sulfonated tetraamine and the corresponding sulfonated polybenzimidazoles (sPBI) were synthesized. For the sake of determining the best polymerization conditions, a study involving model compounds was first performed. A strong acid medium was used as polymerization solvent, which allowed to obtain high molecular weight sPBI. A series of polymers with ion exchange capacity (IEC) ranging from 0 to 2.6 mequiv/g were synthesized using a non-sulfonated tetraamine as a comonomer. The chemical structure of those polymers was confirmed by nuclear magnetic resonance (NMR) and Fourier transform infrared (FTIR) as well as by titration. Thermogravimetric analysis (TGA) and viscosity measurement were performed as well. On the other hand, different architectures of the copolymers were prepared, i.e., random, sequenced copolymers, and blends of the homopolymers. The membranes prepared from the sPBI display low water uptake. The ionic conductivities measured in the hydrated state at room temper...

Published
2007

12. Hydrophobic networks for advanced proton conducting membrane: Synthesis, transport properties and chemical stability

Author

Vincent H. Mareau, Fabrice Gouanvé, Odile Fichet, Linda Chikh, Sylvain Magana, Matthieu Fumagalli, Nicolas Festin, Laurent Gonon, Eliane Espuche, Ingénierie des Matériaux Polymères (IMP), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Physico-chimie des Polymères et des Interfaces (LPPI), Fédération INSTITUT DES MATÉRIAUX DE CERGY-PONTOISE (I-MAT), Université de Cergy Pontoise (UCP), Université Paris-Seine-Université Paris-Seine-Université de Cergy Pontoise (UCP), Université Paris-Seine-Université Paris-Seine, Polymères Conducteurs Ioniques (PCI), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), ANR-11-RMNP-0007,MAMEIRIP,MAtériaux Multicouches Echangeurs d'Ions à base de Réseaux Interpénétrés de Polymères(2011), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), and Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Membrane permeability, Fluorinated network, Diffusion, Gas permeability, chemistry.chemical_element, Filtration and Separation, Electrolyte, [CHIM.MATE]Chemical Sciences/Material chemistry, Biochemistry, chemistry.chemical_compound, Ageing, Monomer, Membrane, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Chemical engineering, Polymer chemistry, Water sorption, Fluorine, General Materials Science, Chemical stability, Thermal stability, Physical and Theoretical Chemistry
Abstract

International audience; The design of interpenetrated networks (IPN) membranes for fuel cell applications requires both an electrolyte and a neutral network. The composition and architecture of the latter are of major importance for the final IPN membrane properties. In this work, networks based on a fluorinated diepoxy oligomer (DFODDE) and a non-fluorinated triepoxy monomer (TMPTGE) were synthesized. The network composition was varied from 100% DFODDE to 100% TMPTGE, resulting in an increase of the crosslinking density and concomitantly a decrease of the fluorine content. The curing process was optimized to achieve a total epoxy conversion and the chemical structure of the networks was characterized by Raman and Infrared spectroscopies. The physical, thermal and chemical membrane properties were studied and discussed as a function of the crosslinking density and of the fluorine content. Increasing the crosslinking density led to a decrease of the membrane permeability to oxygen. Water sorption properties depended on both parameters, with a prevailing role of the fluorine content on the water uptake and a major influence of the crosslinking density on the diffusion parameter. The thermal stability increased also with the fluorine content. All materials exhibited a good stability in water at 80 degrees C but a significant weight loss after immersion in a concentrated H2O2 solution. Altogether, these results indicate that networks containing 20% of TMPTGE exhibit an interesting set of properties (low oxygen permeability, high T-g, good chemical and thermal stability) to behave as a neutral partner in an IPN membrane. Moreover, the low water uptake and diffusion rate measured in these networks make them attractive for water barrier membranes.

Published
2015

13. Untangling the condensation network of organosiloxanes on nanoparticles using 2D $^{29}$Si– $^{29}$Si solid-state NMR enhanced by dynamic nuclear polarization

Author

Nghia Tuan Duong, Guillaume Monin, Daniel Lee, Isabel Zamanillo Lopez, Laurent Gonon, Michel Bardet, Vincent H. Mareau, Gaël De Paëpe, Service de Chimie Inorganique et Biologique (SCIB - UMR E3), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Centre National de la Recherche Scientifique (CNRS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), the 'programme chaire d’excellence' (ANR08-CEXC-003-01), ANR-11-LABX-0003,ARCANE,Grenoble, une chimie bio-motivée(2011), ANR-12-BS08-0016,CryoMAS4DNP,Polarisation dynamique nucléaire en rotation à l'angle magique à très basse température et à haut champ magnétique(2012), European Project: 228664,EC:FP7:PEOPLE,FP7-PEOPLE-2007-2-3-COFUND,EUROTALENTS(2009), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Nanosciences et Cryogénie (INAC), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])

Subjects
Chemistry, Condensation, Analytical chemistry, Nanoparticle, General Chemistry, Biochemistry, Catalysis, Homonuclear molecule, Isotopic labeling, Colloid and Surface Chemistry, Solid-state nuclear magnetic resonance, Polymerization, Silanization, Magic angle spinning, [CHIM]Chemical Sciences
Abstract

International audience; Silica (SiO$_2$) nanoparticles (NPs) were func-tionalized by silanization to produce a surface covered with organosiloxanes. Information about the surface coverage and the nature, if any, of organosiloxane polymerization, whether parallel or perpendicular to the surface, is highly desired. To this extent, two-dimensional homonuclear $^{29}$Si solid-state NMR could be employed. However, owing to the sensitivity limitations associated with the low natural abundance (4.7%) of $^{29}$Si and the difficulty and expense of isotopic labeling here, this technique would usually be deemed impracticable. Nevertheless, we show that recent developments in the field of dynamic nuclear polarization under magic angle spinning (MAS-DNP) could be used to dramatically increase the sensitivity of the NMR experiments, resulting in a timesaving factor of ∼625 compared to conventional solid-state NMR. This allowed the acquisition of previously infeasible data. Using both through-space and through-bond 2D $^{29}$Si− $^{29}$Si correlation experiments, it is shown that the required reaction conditions favor lateral polymerization and domain growth. Moreover, the natural abundance correlation experiments permitted the estimation of $^2J^{Si−O−Si}$-couplings (13.8 ± 1.4 Hz for surface silica) and interatomic distances (3.04 ± 0.08 Å for surface silica) since complications associated with many-spin systems and also sensitivity were avoided. The work detailed herein not only demonstrates the possibility of using MAS-DNP to greatly facilitate the acquisition of 2D $^{29}$Si− $^{29}$Si correlation spectra but also shows that this technique can be used in a routine fashion to characterize surface grafting networks and gain structural constraints, which can be related to a system's chemical and physical properties.

Published
2014

14. Hydrolytic degradation of sulfonated polyimide membranes for fuel cells

Author

Carine Perrot, Gérard Gebel, Laurent Gonon, Catherine Marestin, Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Ingénierie des Matériaux Polymères (IMP), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Jean Monnet [Saint-Étienne] (UJM)-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Université de Lyon-Institut National des Sciences Appliquées (INSA)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon, Département des Technologies des NanoMatériaux (DTNM), Laboratoire d'Innovation pour les Technologies des Energies Nouvelles et les nanomatériaux (LITEN), Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Institut National de L'Energie Solaire (INES), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), and Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Ionic bonding, Filtration and Separation, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Biochemistry, 0104 chemical sciences, chemistry.chemical_compound, Hydrolysis, Monomer, Membrane, chemistry, Polymer chemistry, Copolymer, Degradation (geology), [CHIM]Chemical Sciences, General Materials Science, Physical and Theoretical Chemistry, 0210 nano-technology, Imide, Polyimide, ComputingMilieux_MISCELLANEOUS
Abstract

The hydrolytic degradation mechanism of sulfonated polyimide (sPI) membranes was determined through the study of model compounds and validated with a fully sulfonated polymer. Two model compounds characteristic of the ionic sequence and of the junction between ionic and neutral sequences in block copolymers were synthesized and aged in water at different temperatures. Liquid chromatography was used to separate and identify the degradation products by means of various spectroscopies (IR, UV, NMR). It is shown that the hydrolysis of the naphthalenic imide rings is an equilibrated reaction and that the imide rings are more stable when located between ionic substituted monomer than in the hydrophilic–hydrophobic junctions. It is concluded that block copolymers with long ionic sequences or blends of sulfonated and non sulfonated homopolymers should be more stable than random copolymers. This conclusion is confirmed by the study of the hydrolytic degradation of fully sulfonated polyimide.

Published
2011

15. Degradation of a sulfonated aryl ether ketone model compound in oxidative media (sPAEK)

Author

Alain Pierre-Bayle, Catherine Marestin, Gérard Gebel, Carine Perrot, Michel Bardet, Laurent Gonon, Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Matériaux organiques à propriétés spécifiques (LMOPS), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI ), Institut de Chimie du CNRS (INC)-Institut National Polytechnique de Grenoble (INPG)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut National Polytechnique de Grenoble (INPG)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), and Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
Ketone, Polymers and Plastics, polymer degradation, Proton exchange membrane fuel cell, Ether, sPAEK, 02 engineering and technology, fuel cells, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, Polymer degradation, Polymer chemistry, Materials Chemistry, Organic chemistry, Hydrogen peroxide, ComputingMilieux_MISCELLANEOUS, chemistry.chemical_classification, Chemistry, Aryl, Organic Chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Membrane, [CHIM.POLY]Chemical Sciences/Polymers, Hydroxyl radical, 0210 nano-technology
Abstract

Poor durability of polymer electrolyte membranes is one of the most limiting factors of proton exchange membrane fuel cell (PEMFC). Hydrogen peroxide which is formed electrochemically or chemically during operation is one of the potential deteriorating factors, particularly for polyaromatic membranes. To be able to increase membrane durability, the aging path involved must be elucidated. To give an insight into the degradation mechanism of sulfonated polyaryl ether ketones (sPAEK) a study on model compound has been performed. Each species produced has been collected by liquid chromatography and identified by NMR, IR and mass spectroscopies. We have demonstrated that degradation proceeds through the addition of a hydroxyl radical on the aromatic ring. Then, the oxidation of these phenolic groups leads to several chain scissions. On the basis of these experiments, a strategy can be drawn to improve the membrane durability.

Published
2009

16. Ex situ hydrolytic degradation of sulfonated polyimide membranes for fuel cells

Author

Sandrine Morlat, Laurent Gonon, Gilles Meyer, Carine Perrot, Gérard Gebel, Jean-Luc Gardette, Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Photochimie moléculaire et macromoléculaire (PMM), Université Blaise Pascal - Clermont-Ferrand 2 (UBP)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie de Clermont-Ferrand (ICCF), and Université Blaise Pascal - Clermont-Ferrand 2 (UBP)-SIGMA Clermont (SIGMA Clermont)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
chemistry.chemical_classification, Polymers and Plastics, Organic Chemistry, Infrared spectroscopy, 02 engineering and technology, Polymer, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, chemistry.chemical_compound, Hydrolysis, Monomer, Membrane, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Chemical engineering, Polymer chemistry, Materials Chemistry, 0210 nano-technology, Imide, Hydrogen peroxide, Polyimide
Abstract

Ex situ hydrolytic stability of sulfonated polyimide (s-PI) membranes for fuel cells was studied depending on structural and external parameters including the ion exchange capacity, the block character, the temperature and the hydrogen peroxide concentration. Infrared spectroscopy was used to identify and quantify the chemical modifications such as the loss of imide functions and of ionic monomers. The decrease in ion exchange capacity due to the elution of sulfonated oligomers was confirmed by sulfur content analysis. A complete hydrolysis of some of the imide functions is observed leading to polymer chain scissions and to the loss of the mechanical properties. It is shown to be a thermo activated process and the activation energy (60 kJ/mol) is found in good agreement with the value determined from fuel cell lifetimes. The degradation in fuel cell conditions is similar but faster than in pure water. The same kinetic can be reproduced ex situ by addition 0.05% of hydrogen peroxide.

Published
2006

17. Degradation of sulfonated polyimide membranes in fuel cell conditions

Author

Gilles Meyer, Philipe Capron, Régis Mercier, Gérard Gebel, Catherine Marestin, Didier Marscaq, Laurent Gonon, Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Institut Nanosciences et Cryogénie (INAC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Matériaux organiques à propriétés spécifiques (LMOPS), Laboratoire d'Electrochimie et de Physico-chimie des Matériaux et des Interfaces (LEPMI ), Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Institut de Chimie du CNRS (INC)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), and Institut de Chimie du CNRS (INC)-Institut National Polytechnique de Grenoble (INPG)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut National Polytechnique de Grenoble (INPG)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Analytical chemistry, Energy Engineering and Power Technology, Infrared spectroscopy, 02 engineering and technology, Activation energy, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, Nafion, Electrical and Electronic Engineering, Physical and Theoretical Chemistry, Fuel cells, Chemical decomposition, ComputingMilieux_MISCELLANEOUS, degradation, chemistry.chemical_classification, Renewable Energy, Sustainability and the Environment, Polymer, sulfonated polyimide, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Membrane, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Chemical engineering, Degradation (geology), proton conducting membranes, 0210 nano-technology, Polyimide
Abstract

The stability of sulfonated polyimide (sPI) membranes in fuel cell conditions was studied under stationary and cycling electric loading conditions. The lifetime in operating conditions was shown to vary from few tens to several hundreds of hours depending on both the membrane ion content and the fuel cell temperature. The membrane degradation is shown to be a thermoactivated process and activation energies have been extracted (70–110 kJ). The membrane post-mortem analysis by infrared revealed a significant chemical degradation which was identified as the imide function hydrolysis inducing polymer chain scissions and consequently the loss of the mechanical properties. In addition to this main degradation process, the infrared analysis of the membrane surface exposed to the anodic compartment suggests the occurrence an additional oxidative process. sPI membranes exhibit a lower sensitivity to operation under electric loading cycling compared to Nafion.

Published
2006

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